CN111790437B - Strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by liquid phase method ethanol and preparation method and application thereof - Google Patents
Strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by liquid phase method ethanol and preparation method and application thereof Download PDFInfo
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2529/00—Catalysts comprising molecular sieves
- C07C2529/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
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- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method, which comprises 1-5 parts of strontium, 1-3 parts of tantalum and the balance of Ti-MWW molecular sieve according to 100 parts by weight; meanwhile, the invention also discloses a preparation method of the catalyst and application of the catalyst in preparation of 2-pentanone from ethanol by a liquid phase method. When the catalyst provided by the invention is used for preparing 2-pentanone, cheap coal-based ethanol is used as a raw material, so that the raw material cost is low; the strontium-tantalum-titanium trimetal oxide is used as a catalyst, raw material ethanol is used as a solvent, 2-pentanone is prepared in a slurry bed reactor in a high selectivity of liquid and solid phases, the conversion rate of the ethanol is more than 80%, and the selectivity of the product 2-pentanone is more than 70%.
Description
Technical Field
The invention belongs to the technical field of industrial catalysis, and particularly relates to a strontium-tantalum-titanium trimetallic oxide catalyst for preparing 2-pentanone from ethanol by a liquid phase method, and a preparation method and application thereof.
Background
Methyl propyl ketone (2-pentanone), also known as 2-pentanone, is a colorless liquid of chemical synthesis. The main application of the compound is to serve as an industrial solvent, and the compound can be widely used for manufacturing various oil-resistant gaskets, rubber tubes, airplane fuel tanks, flexible packages, printing and dyeing rubber rollers, cable materials, adhesives and the like, can also serve as an organic synthesis intermediate and a medical synthesis intermediate, and can be used for synthesizing vasodilator drugs Virga. 2-pentanone is also an excellent organic solvent, can be used as an excellent dewaxing agent of lubricating oil, a solvent of nitro spray paint and synthetic resin coating, can be used as an extracting agent and the like, and is an indispensable elastic material in the industries of automobiles, aviation, petroleum, copying and the like.
The 2-pentanone can be prepared by the ammoxidation of butene and can also be prepared by the catalysis of butanol and ammonia, and the traditional 2-pentanone synthesis method is the oxidative dehydrogenation of 2-pentanol or the co-heating of butyrylacetic acid ethyl ester and water. Chinese patents CN 1660749A and CN 1660750A disclose K-Pd/ZrO 2 Catalyst of/MnO/ZnO, which can be used for synthesizing 2-pentanone from ethanolHowever, the catalyst component in the process is complex and difficult to regulate and control; meanwhile, the use of noble metals and the catalytic reaction process need to be carried out under certain pressure, and the like. Chinese patent CN 106478386A discloses a new type of CeO 2 As a catalyst, the method for preparing 2-pentanone from ethanol has the problems of overhigh reaction temperature, low product selectivity and the like.
At present, various 2-pentanone production methods have the problems of serious three-waste pollution, low product selectivity, difficult product separation and purification and the like. If the 2-pentanone can be prepared by the ethanol liquid phase one-step method at low temperature and normal pressure with high selectivity, the production cost and equipment investment are greatly reduced, the process flow is simplified, and a green, environment-friendly and competitive production route is realized.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by using liquid phase ethanol and the preparation method thereof, and simultaneously provides the application of the catalyst in preparing 2-pentanone, so that the 2-pentanone can be prepared with high selectivity, the reaction condition is mild, and the cost is low.
The strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by using ethanol through a liquid phase method comprises, by weight, 100 parts of strontium 1-5 parts, 1-3 parts of tantalum and the balance of a Ti-MWW molecular sieve.
Preferably, the catalyst consists of 5 parts of strontium, 1 part of tantalum and 94 parts of Ti-MWW molecular sieve.
The Ti-MWW molecular sieve is prepared by adopting the prior art.
The preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method comprises the following steps:
(1) grinding the Ti-MWW molecular sieve for later use;
(2) at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine being 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine being 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
(3) adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 12-48h at room temperature, and then heating to 60-90 ℃ for secondary purification for 6-12 h;
(4) filtering, washing with distilled water of the same volume for 2-5 times, drying, roasting, and naturally cooling to obtain the catalyst.
Preferably, the drying conditions are drying at 110-140 ℃ for 4-6 h.
Preferably, the roasting condition is roasting at 500-550 ℃ for 4-12 h.
A method for preparing 2-pentanone from ethanol by a liquid phase method comprises the following specific steps: filling catalyst in a slurry bed reactor to form a catalyst bed layer, taking ethanol as a raw material, and reacting at the temperature of 50-60 ℃, under the normal pressure and at the weight space velocity of 0.1-1h -1 Introducing the mixed solution into the slurry bed reactor under the condition of (1), and rectifying the mixed solution to obtain 2-pentanone through the catalyst bed layer; the unreacted ethanol after rectification is circulated back to the slurry bed reactor;
wherein, the catalyst is the catalyst of the invention.
Preferably, the method for preparing 2-pentanone by using liquid phase ethanol comprises the following steps of filling a catalyst in a slurry bed reactor to form a catalyst bed layer, taking ethanol as a raw material, and reacting at 60 ℃ under normal pressure at a weight space velocity of 0.1h -1 Introducing the mixed solution into the slurry bed reactor under the condition of (1), and rectifying the mixed solution to obtain 2-pentanone through the catalyst bed layer; the unreacted ethanol after rectification is circulated back to the slurry bed reactor.
The invention has the advantages that:
(1) when the catalyst provided by the invention is used for preparing 2-pentanone, cheap coal-based ethanol is used as a raw material, so that the raw material cost is low; the strontium-tantalum-titanium trimetal oxide is used as a catalyst, raw material ethanol is used as a solvent, 2-pentanone is prepared in a slurry bed reactor in a high selectivity of liquid and solid phases, the conversion rate of the ethanol is more than 80%, and the selectivity of the product 2-pentanone is more than 70%;
(2) when the 2-pentanone is prepared, the raw materials have no toxicity, the preparation process has no three-waste discharge, and the environmental pollution is small;
(3) when 2-pentanone is prepared, ethanol is used as a raw material and a solvent, and simultaneously, because the trimetal oxide meets the effects of a molecular sieve and the solvent, the possibility of ethanol disproportionation to other products is reduced, the generation of byproducts is reduced, the catalytic reaction under normal pressure is realized, the reaction condition is mild, and the equipment investment and the operation cost are reduced; the selectivity of 2-pentanone is improved by utilizing the molecular sieve shape selection effect, the reaction product composition is simple, and the separation and purification process cost is low.
Detailed Description
Example 1
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by liquid phase method ethanol comprises 5 parts of strontium, 1 part of tantalum and 94 parts of Ti-MWW molecular sieve; the catalyst number is YCSY-01;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method comprises the following steps:
(1) grinding the Ti-MWW molecular sieve for later use;
(2) at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
(3) adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 24 hours at room temperature, and then heating to 80 ℃ for secondary purification for 8 hours;
(4) filtering, washing with distilled water of the same volume for 5 times, drying at 120 ℃ for 5h, roasting at 550 ℃ for 10h, and naturally cooling to obtain the catalyst.
Example 2
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by liquid phase method ethanol comprises 5 parts of strontium, 3 parts of tantalum and 92 parts of Ti-MWW molecular sieve; the catalyst is numbered YCSY-02;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method comprises the following steps:
(1) grinding the Ti-MWW molecular sieve for later use;
(2) at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
(3) adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 12h at room temperature, and then heating to 60 ℃ for secondary purification for 12 h;
(4) filtering, washing with distilled water of the same volume for 2 times, drying at 110 ℃ for 6 hours, roasting at 500 ℃ for 12 hours, and naturally cooling to obtain the catalyst.
Example 3
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method is composed of 2 parts of strontium, 1 part of tantalum and 97 parts of Ti-MWW molecular sieve; the catalyst is numbered YCSY-03;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method comprises the following steps:
(1) grinding the Ti-MWW molecular sieve for later use;
(2) at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
(3) adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 48 hours at room temperature, and then heating to 90 ℃ for secondary purification for 6 hours;
(4) filtering, washing with distilled water of the same volume for 5 times, drying at 140 ℃ for 4h, roasting at 550 ℃ for 4h, and naturally cooling to obtain the catalyst.
Example 4
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method is composed of 4 parts of strontium, 1 part of tantalum and 95 parts of Ti-MWW molecular sieve; the catalyst number is YCSY-04;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method comprises the following steps:
(1) grinding the Ti-MWW molecular sieve for later use;
(2) at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
(3) adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 36h at room temperature, and then heating to 75 ℃ for secondary purification for 9 h;
(4) filtering, washing with distilled water of the same volume for 4 times, drying at 120 ℃ for 5h, roasting at 500 ℃ for 8h, and naturally cooling to obtain the catalyst.
Example 5
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method is composed of 2 parts of strontium, 2 parts of tantalum and 96 parts of Ti-MWW molecular sieve; the catalyst number is YCSY-05;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through the liquid phase method is the same as that of example 4.
Example 6
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by using ethanol through a liquid phase method is composed of 2 parts of strontium, 3 parts of tantalum and 95 parts of Ti-MWW molecular sieve; the catalyst is numbered YCSY-06;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through the liquid phase method is the same as that of example 4.
Example 7
A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method is composed of 1 part of strontium, 1 part of tantalum and 98 parts of Ti-MWW molecular sieve; catalyst number YCSY-07;
the preparation method of the strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through the liquid phase method is the same as that of example 4.
Applications of
The catalyst prepared by the embodiment of the invention is applied to the liquid phase method for preparing 2-pentanone by ethanol, and the specific preparation method is as follows: the catalyst prepared by the embodiment of the invention is filled in a slurry bed reactor to form a catalyst bed layer, ethanol is used as a raw material, the reaction temperature is 50-60 ℃, the reaction pressure is normal pressure, and the weight space velocity is 0.1-1h -1 Introducing the mixed solution into the slurry bed reactor under the condition of (1), and rectifying the mixed solution to obtain 2-pentanone through the catalyst bed layer; the unreacted ethanol after rectification is circulated back to the slurry bed reactor; the catalytic performance of the catalyst was evaluated, and the specific reaction conditions and results are shown in table 1.
TABLE 1 reaction conditions and results
Claims (7)
1. A strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone by ethanol through a liquid phase method is characterized in that: the catalyst consists of 1-5 parts of strontium, 1-3 parts of tantalum and the balance of Ti-MWW molecular sieve according to 100 parts by weight;
the catalyst is prepared by the following method:
grinding the Ti-MWW molecular sieve for later use;
at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 12-48h at room temperature, and then heating to 60-90 ℃ for secondary purification for 6-12 h;
filtering, washing with distilled water of the same volume for 2-5 times, drying, roasting, and naturally cooling to obtain the catalyst.
2. The strontium-tantalum-titanium trimetal oxide catalyst for preparing 2-pentanone from ethanol by the liquid phase method according to claim 1, wherein the strontium-tantalum-titanium trimetal oxide catalyst is characterized in that: the catalyst consists of 5 parts of strontium, 1 part of tantalum and 94 parts of Ti-MWW molecular sieve.
3. A process for preparing the catalyst of claim 1 or 2, characterized in that: the method comprises the following steps:
grinding the Ti-MWW molecular sieve for later use;
at the isoelectric point of taurine, adding strontium carbonate into an aqueous solution of taurine according to the molar ratio of strontium atoms to taurine of 1:1 to obtain a strontium carbonate-taurine mixed solution, and simultaneously adding tantalum carbonate into an aqueous solution of taurine according to the molar ratio of tantalum atoms to taurine of 1:1 to obtain a tantalum carbonate-taurine mixed solution; then mixing the strontium carbonate-taurine mixed solution with the tantalum carbonate-taurine mixed solution, and adjusting the pH of the mixed solution to taurine isoelectric point by using dilute hydrochloric acid to obtain an amino acid metal complex solution;
adding a ground Ti-MWW molecular sieve into the amino acid metal complex solution, soaking for 12-48h at room temperature, and then heating to 60-90 ℃ for secondary purification for 6-12 h;
filtering, washing with distilled water of the same volume for 2-5 times, drying, roasting, and naturally cooling to obtain the catalyst.
4. The method for preparing the catalyst according to claim 3, wherein: the drying condition is drying at 110-140 ℃ for 4-6 h.
5. The method for preparing the catalyst according to claim 4, wherein: the roasting condition is roasting for 4-12h at 500-550 ℃.
6. A method for preparing 2-pentanone from ethanol by a liquid phase method is characterized by comprising the following steps: the method comprises the following steps: filling a catalyst in a slurry bed reactor to form a catalyst bed layer, taking ethanol as a raw material, and reacting at the temperature of 50-60 ℃, the reaction pressure of normal pressure and the weight space velocity of 0.1-1h -1 Introducing the mixed solution into the slurry bed reactor under the condition of (1), and rectifying the mixed solution to obtain 2-pentanone through the catalyst bed layer;
wherein the catalyst is the catalyst of claim 1.
7. The method for preparing 2-pentanone from ethanol by using the liquid phase method according to claim 6, wherein the method comprises the following steps: the method comprises the following steps: filling a catalyst in a slurry bed reactor to form a catalyst bed layer, taking ethanol as a raw material, and reacting at the temperature of 60 ℃, the reaction pressure of normal pressure and the weight space velocity of 0.1h -1 Introducing the mixed solution into the slurry bed reactor under the condition of (1), and rectifying the mixed solution to obtain 2-pentanone through the catalyst bed layer.
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| CN111389457A (en) * | 2020-04-22 | 2020-07-10 | 陕西延长石油（集团）有限责任公司 | Catalyst and method for preparing methacrylic acid and propylene oxide by co-oxidation of isobutane and propylene |
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